Synthesis and Crystal Structure of a One-dimensional Infinite Chain Organotin Complex [(n-Bu)_3Sn(OCOC_5H_4NO)]_n

A novel organotin complex [（n-Bu）3Sn（OCOC5H4NO）]n has been synthesized and characterized by elemental analysis, IR and ^1H NMR. The crystal structure has been determined by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P2 1/c with a = 8.982（2）, b = 17.908（4）, c = 13.219（3） A, β= 96.981（4）°, Z = 4, V= 2110.6（8） A^3, Dc = 1.347 g/cm^3, μ（MoKa） = 12.23 cm^-1, F（000） = 880, R = 0.0497 and wR = 0.1263. In the molecular structure of the title complex, the tin atoms are five-coordinated in a distorted trigonal bipyramidal geometry. A one-dimensional linear polymer is formed through an interaction between the O atoms of pyridine-3-carboxylic acid N-oxide and tin atoms of an adjacent molecule.

Synthesis and Crystal Structure of a Novel Mercapto-organotin Complex: [Et_3NH] [Ph_2SnCl(μ~2-SCH_2COO^-)]

A novel complex [Et3NH] [Ph2SnCl(μ2- SCH2COO-)] has been unexpectedly obtained by the reaction of Ph3SnCl and HSCH2COOH in 2:1 molar ratio in the presence of organic base Et3N. Possible dephenylation mechanism was illustrated. The X-ray diffraction study has shown that the title complex consists of cation moiety [Et3NH] and anion moiety [Ph2SnCl(μ2 - SCH2COO)] with tin(IV) in a trigonal bipyramidal coordination geometry.

Crystal Structure of A Novel Ionic Organotin Complex:{[Ph_(2)Sn]_(2)[2,6-(O_(2)C)_(2)C_(5)H_(3)N]_(3)H_(2)O}^(2-)[HNEt_(3)]_(2)^(+)

A novel ionic organotin complex{[Ph_(2)Sn]_(2)[2,6-(O_(2)C)_(2)]C_(5)H_(3)N}_(3)H_(2)O}^(2-)[HNEt_(3)]^(2+)has been unexpectedly obtained by the reaction of Ph_(3)SnCl and 2,6-pyridine dicarboxylic acid in 1:1 molar ratio in the presence of organic base Et_(3)N.Possible dephenylation mechanism was illustrated.The X-ray diffraction study has shown that the title complex consists of cation moiety[HNEt_(3)]^(+)and anion moiety{[Ph_(2)Sn]_(2)[2,6-(O_(2)C_(2))C_(5)H_(3)N]_(3)H_(2)O}^(2-)with tin(IV)in a pengonal bipyramidal coordination geometry.

Diorganotin Complexes of N-[4-(Diethylamino)salicylidene]-(L)-tryptophane: Syntheses, Structures and Properties

Four chiral diorganotin complexes of N-[4-(diethylamino)salicylidene]-(L)-tryptophane,R2Sn[4-(Et2N)-2-OC6H3CH=NCH(CH2Ind)COO](Ind=3-indolyl;R=Me(1);Et,(2);n-Bu(3);Cy(cyclohexyl)(4)),have been synthesized and characterized by elemental analysis,IR,and 1H and 13C NMR spectra.The crystal structures of 1-CH3OH-CHCl3,2,3-CH3OH and 4-CH3CH2OH have been determined by single-crystal X-ray diffraction.The complexes crystallize in orthorhombic system with P212121 space group,and the tin atoms are in distorted trigonal bipyramidal geometry and form five-and six-membered chelate rings with the chiral ONO tridentate ligand N-[4-(diethylamino)salicylidene]-(L)-tryptophane.In the complexes,the molecules are connected into one-dimensional supramolecular chain by intermolecular N–H…O–H…O=C or N–H…O–C hydrogen bonds.The fluorescence spectrum indicates that the complexes may be explored for potential blue luminescent materials.Bioassay results show that 3 and 4 belong to the efficient cytostatic agents against A549 human tumor cell.

Synthesis and Anion Recognition of a Novel Heterocyclic Organotin Complex

A novel heterocyclic hexacoordinate organotin(Ⅳ) complex, bis(O-vanillin)-semi ethylenediamino dibenzyltin (VEDBT) was synthesized by the reaction of dibenzyltin dichloride with bis(O-vanillin)-semiethyenediamine, its structure has been characterized by spectral methods. The electrodes using VEDBT as a neutral carrier show high selectivity for salicylate anions.

Formation,Structure and In Vitro Antitumour Activity of a Novel Binuclear Organotin Complex

A 1：1 reaction of triphenyltin chloride with potassium N-[（3,5-dibromo-2-hydroxylphenyl）methylene]valinate in benzene led to the formation of a novel mixed organotin dinuclear complex, （HL）SnPh3oPh2SnL [L=2-O-3,5-Br2C6H3CH=NCH（i-Pr）COO], by means of a facile phenyl-tin bond cleavage process. In the complex, there are two distinct types of carboxylate moieties and a trans-O2SnC2N and a trans-O2SnC3 in distorted trigonal bipyramidal geometries were bridged by a carboxylate group. In vitro antitumor activity of the complex against three human tumour cell lines （HeLa, CoLo205 and MCF-7） was found to be much higher than cis-platin used in clinic.

Synthesis, Properties and Crystal Structure of Seven-coordinated Organotin Complex [~nBu_2Sn(OOCC_5H_4N-2)_2(H_2O)]

A novel seven-coordinated organotin complex [ nBu 2Sn-(OOCC 5H 4N-2) 2(H 2O)] was unexpectedly synthesized by reaction of nBu 3SnCl with 2-pyridinecarboxylic acid in 1∶1 molar ratio in the presence of organic base Et 3N. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to rhombohedral with space group R-3c, a=1.5807(3) nm, b=1.5807(3) nm, c=1.5807(3) nm, α=105.717(2)°, β=105.717(2)°, γ=105.717(2)°, Z=6, V=3.397(8) nm 3, D c=1.452 g/cm 3, μ=1.158 mm -1, F(000)=1512, R 1=0.0447, wR 2=0.1038. In crystal, the tin atoms rendered seven-coordinate in a distorted pentagonal bipyramidal geometry. The two-dimensional network structure was formed by H-bonding interaction between the free oxygen atoms of carboxyl groups and the coordinated water molecules.

Synthesis,Structure and Biological Activities of a Novel Anionic Organotin(Ⅳ)Complex{[(pClC6H4CH2)Sn(H2O)(Cl)2OCOCH(O)CH(O)CO2Sn(H2O)(Cl)2(p-ClC6H4CH2)]·2(HNEt3)}

A novel anionic organotin(Ⅳ) complex {[(pClCHCH)Sn(HO)(Cl)OCOCH(O)CH(O)COSn(HO)(Cl)(p-ClCHCH)]·2(HNEt)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar in the presence of an organic base triethylamine. The structure was characterized by elemental analysis, IR, TG, XRD and single-crystal X-ray diffraction. It crystallizes in triclinic, P1 space group, with a = 0.7067(1), b = 1.9762(3), c = 2.2383(3) nm, α = 91.544(2)°, β = 90.075(2)°, γ = 90.110(2)°, V = 3.1247(7) nm~3, Z = 3, Dc = 1.621 g/cm~3, m(Mo Kα) = 16.29 cm–1, F(000) = 1530, R = 0.0394, wR = 0.1092,(Δρ)max = 1224 and(Δρ)min = –840 e/nm~3. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of 1 have been carefully investigated with quantum chemistry calculation. In addition, the in vitro antitumor activity suggested that 1 had stronger inhibitory activity on H460, MCF7 than on A549.

Synthesis, spectral characterization and biological activities of Organotin(IV) complexes with <i>ortho</i>-vanillin-2-hydrazinopyridine (VHP)

Five new organotin(IV) complexes of ortho-vanillin-2-hydrazinopyridine hydrazone with formula [RnSnCl4–n(VHP)] [R = Me2, n = 2 (2);R = Ph2, n = 2 (3);R= nBu2, n = 2 (4);R = nBu, n = 2 (5) and R = 1, n = 0 (6)] have been synthesized by direct reaction of ortho-vanillin-2-hydrazinopyridine hydrazone [(VHP), (1)], base and organotin(IV) chloride(s) in absolute methanol. The hydrazone ligand [(VHP), (1)] and its organotin(IV) complexes (2-6) have been characterized by UV-Visible, FT-IR and 1H NMR spectral studies. Spectroscopic data suggested that in the complexes (2-4), the ligand (1) acted as a neutral bidentate ligand and is coordinated to the tin(IV) atom via the azomethine nitrogen and pyridyl nitrogen atoms, whereas the ligand (1) acted as a uninegative tridentate ligand and coordinated to the tin(IV) atom through phenolic-O, azomethine-N and pyridyl-N atoms in complexes (5-6). The toxicity of the ligand (1) and its organotin (IV) complexes (2-6) were determined against Artemia salina. Organotin(IV) complexes showed moderate activity against Artemia salina. The ligand (1) and its organotin(IV) complexes (2-6) were also tested against four types of bacteria namely Bacillus cereus, Staphylococcus aureus, Escherichia coli and Enterobacter aerogenes. All organotin(IV) complexes and the free ligand (1) showed better antibacterial activities against bacteria. Among the organotin(IV) complexes (2-6), diphenyltin(IV) complex (3) showed higher activity against the four types of bacteria.

Synthesis, Characterization and Antibacterial Activity of Cyclohexyltin Complexes of N-(3,5-Dibromosalicylidene)valine

Three cyclohexyltin complexes of N-（3,5-dibromosalicylidene）valine（H_2L）, Cy_3Sn（HL）（1）, Cy_2SnL（2）, and Cy2 SnL ·Cy_3Sn Cl（3）（Cy = cyclohexyl）, have been synthesized and characterized by elemental analysis, IR, and ~1H and ^（13） C NMR spectra. The crystal structures of 2 and 3 have been determined. Complex 2 belongs to the monoclinic system, space group P21/n with a = 21.250（8）, b = 10.837（4）, c = 23.050（8） ？, b = 93.193（9）°, V = 5300（3） ？~3, Z = 8, D_c = 1.659 g/cm^3, m = 4.004 mm^（-1）, F（000） = 2624, R = 0.0471 and wR = 0.1015. Complex 3 belongs to the monoclinic system, space group P21 with a = 10.3452（10）, b = 18.7665（18）, c = 12.1483（12） ？, b = 103.374（2）°, V = 2294.5（4） ？3, Z = 2, D_c = 1.542 g/cm^3, m = 2.923 mm^（-1）, F（000） = 1072, R = 0.0428 and wR = 0.0936. Complex 2 has a distorted trigonal bipyramidal geometry with the axial locations occupied by one carboxylate oxygen and a phenolic oxygen of the ligand, and 3 reveals that the two tin atoms are joined via the carbonyl atom of the ligand to form a mixed organotin binuclear complex. Bioassay results show that 1 and 2 have good in vitro antibacterial activity against Escherichia coli.

Syntheses and Structural Characterization of Dimethyltin Complexs of N-(3-Methoxysalicylidene)-α-amino Acid

Three new dimethyltin complexes of N-（3-methoxysalicylidene）-α-amino acid,（CH3）2Sn（3-CH3O-2-OC6H3CH=NCHRCOO）（R = H,1;CH3,2;（CH3）2CH,3）,have been synthe-sized by treating dimethyltin dichloride with the potassium salt of the ligand and characterized by elemental analysis,IR and 1H NMR spectra.The crystal structure of [（CH3）2Sn（3-CH3O-2-OC6H3CH=NCH2COO）（CH3OH）]2 H2O（1a）,formed from methanol solution of 1,has been deter-mined.The crystal belongs to the monoclinic system,space group C/2c with a = 20.636（3）,b = 7.8854（9）,c = 20.668（2） ,β= 113.265（2）°,V = 3089.7（6） 3,Z = 4,Dc = 1.707 g/cm3,= 1.675 mm-1,F（000） = 1592,R = 0.0301 and wR = 0.0841.In complex 1a,the tin atom is six-coordinate and possesses a distorted [SnC2NO3] octahedral geometry with the two methyl groups occupying the trans positions.The weak Sn O interactions and intermolecular hydrogen bonds connected the molecules into an infinite chain.

Synthesis,Characterization and Crystal Structure of the Dimeric Organotin Compound:{[n-Bu_(2)Sn(O_(2)CCH_(2)CS_(2)NC_(4)H_(8))]_(2)O}_(2)

The title compound,{[n-Bu_(2)Sn(O_(2)CCH_(2)CS_(2)NC_(4)H_(8))]_(2)O}_(2),has been synthesized by the reaction of(tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in1∶1molar ratio.The complex has been characterized by elemental analysis,IR and NMR.The crystal structure of it has been determined by X-ray single crystal diffraction.And the results showed that the crystal belongs to triclinic system with space group P1and some crystal parameters:a=1.2202(9)nm,b=1.3158(10)nm,c=1.3804(10)nm,α=111.215(9)°,β=99.357(9)°,γ=96.075(10)°,V=2.006(2)nm 3,Z=1,F(000)=908,μ=1.489mm^(-1),D c=1.474g·cm^(-3),R_(1)=0.0375,wR_(2)=0.0839.The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn_(2)O_(2)unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron.Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen.Four carboxylate ligands are divided into two types.And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms,whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only.CCDC:220513.

Syntheses and Crystal Structures of Two Diethyltin Complexes of N-Salicylidene-α-amino Acid

Two novel diethyltin（IV） complexes of N-salicylidenevaline （H2L1） and N-Sali- cylidenetryptophan （H2L^2）, Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730（5）, c = 23.6890（13）A^°, V= 7620.4（5） A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F（000） = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550（8）, b = 11.5425（7）, c = 12.7876（7）A^°, β= 93.585（1）°, V = 2026.3（2） A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F（000） = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.

Synthesis, Crystal Structure, and Thermal Stability of a Dibutyltin Complex {[4-Et_2NC_6H_3(O)C=NC_6H_3(O)-5-NO_2](n-Bu_2Sn)}_2 and Its Interaction with DNA

The Schiff base organotin（IV） complex {[4-Et2NC6H3（O）C=NC6H3（O）-5-NO2]（n- Bu2Sn）}2 has been synthesized via the reaction between 4-（diethylamino） salicylaldehyde-2-arnino- 4-nitrophenol Schiff base （H2L） and dibutyltin oxide. Complex C1 has been characterized by IR, 1H NMR, 13C NMR spectra, and elemental analysis, and its crystal structure was determined by X-ray diffraction, It crystallizes in the monoclinic system, space group P21/n with a = 15.6559（8）, b = 9.1657（5）, c = 18.8351（10） ]A, β = 107.3440（10）°, Z = 4, V = 2579.9（2） A3, Dc = 1.442 Mg.m-3, μ（MoKa） = 1.025 mm-1, F（000） = 1152, R = 0.0250 and wR = 0.0633. The central Sn atom is coordinated in a hexadentate manner to assume a distorted octahedral configuration. Complex C1 was studied by TGA analysis in air atmosphere. The interaction between complex C1 and the herring sperm DNA was realized through the intercalation of the complex based on the studies by EB fluorescent probe.

Syntheses, Crystal Structures and Biological Activities of the 2-Oxo-3-phenylpropionic Acid Arylformylhydrazone Dibenzyltin Complexes

Two 2-oxo-3-phenylpropionic acid arylformylhydrazone dibenzyltin(IV)complexes{[C4H3O(O)C=N-N=C(PhCH2)COO](C6H5CH2)2Sn(CH3OH)}2(Ⅰ)and{[t-Bu-C6H4(O)C=N-N=C(PhCH2)COO](C6H5CH2)2Sn(CH3OH)}2(Ⅱ)have been synthesized and characterized by IR,1H,13C and 119Sn NMR spectra,HRMS,and elemental,thermal stability and single-crystal X-ray diffraction analyses.Complex I crystallizes in the triclinic system,space group P1 with a=9.0392(9),b=10.249(1),c=15.5762(15)?,α=98.605(1)°,β=103.765(1)°,γ=104.056(1)°,Z=2,V=1326.3(2)?3,Dc=1.511 Mg·m^–3,m(MoKa)=1.005 mm–1,F(000)=612,R=0.0206 and wR=0.0524.Complex Ⅱ belongs to triclinic system,space group P1,a=11.4643(3),b=11.8885(3),c=13.0362(4)?,α=73.800(1)°,β=71.679(1)°,γ=79.006(1)°,Z=2,V=1609.34(8)?3,Dc=1.381 Mg·m^–3,m(MoKa)=0.833 mm–1,F(000)=688,R=0.0244 and wR=0.0244.In vitro antitumor activities of both complexes were evaluated by MTT against three human cancer cell lines(NCI-H460,HepG2 and MCF7)and human cell lines(HL7702).Both complexes exhibit better antitumor activity.Furthermore,the interaction between both complexes and calf thymus DNA was studied with EB fluorescent probe.

Synthesis of Five-coordinated Anionic Tin(Ⅳ) Complexes and Crystal Structure of [(i-Pr)_2NH_2][PhSn( μ~2-SCH_2COO)_2]

Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R_ n NH_ 4- n ][PhSn( μ 2-SCH_2COO)_2] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of different organic bases and characterized by means of IR, 1H NMR and MS spectroscopies. The crystal structure of [( i -Pr)_2NH_2] [PhSn( μ 2-SCH_2COO)_2] was determined by X-ray diffraction. In the crystal structure,the tin atom is five-coordinated and exists in trigonal bipyramid geometry with cell parameters a =1.1766(11) nm, b =1.3144(14) nm, c =1.3336(15) nm,β =90° and Z =4.

Synthesis,Crystal Structure and Properties of A Triphenyltin Schiff Complex with Salicylidene-2-aminophenol

The triphenyltin complex with salicylidene-2-aminophenol （C31H24NO2Sn, 1） has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and X-ray single-crystal diffraction. The complex crystallizes in monoclinic system, P21/c space group with a = 1.09515（8）, b = 1.17739（8）, c = 2.29075（14） nm, β = 117.070（4）°, V = 2.6302（3） nm3, Z = 4, Dc = 1.417 g/cm3, ？ = 0.999 mm–1, F（000） = 1123, R = 0.0472 and wR = 0.1169. X-ray single-crystal diffraction showed that 1 demonstrates a one-dimensional chain structure. The quantum chemical calculation of 1 has been investigated. Complex 1 emits fluo- rescence at 558 nm and exhibits certain inhibitory activity against NCI-H460, A549 and MCF-7.

一维链状3-吡啶甲酸三苄基锡的合成和晶体结构

利用三苄基氯化锡和3-吡啶甲酸在三乙胺存在下以1:1摩尔比反应,合成了一维链状的有机锡配合物3-吡啶甲酸三苄基锡{(C7H7)3Sn(PyCO2H)2Sn(C7H7)3}。通过元素分析、红外光谱、核磁共振氢谱和X-射线单晶衍射对其结构进行了表征。测试结果表明:该配合物(C27H25- NO2Sn, Mr = 514.17)为单斜晶系,空间群P21/c, a = 10.618(6), b = 14.683(8), c = 16.050(9) ?β= 106.488(9)? Z = 4, V = 2399(2) ?, Dc = 1.423 g/cm3, ?= 1.087 mm-1, F(000) = 1040, R = 0.0266, wR = 0.0629。通过3-吡啶甲酸配体的氮原子桥联, 形成五配位三角双锥构型的链状结构。

2-羰基-3-苯基丙酸芳甲酰腙二(2,4-二氯苄基)锡配合物的合成、晶体结构及生物活性

二(2,4-二氯苄基)二氯化锡分别与2-羰基-3-苯基丙酸苯甲酰腙及2-羰基-3-苯基丙酸水杨酰腙反应,合成了2个取代苄基锡配合物(C1、C2),通过元素分析、IR、1H NMR、13C NMR、119Sn NMR、X射线单晶衍射以及热重分析等表征了配合物结构。测试了配合物对癌细胞Hela、MCF7、Hep G2、Colo205、NCI-H460以及正常人体胚肾细胞HEK293、正常人体肝细胞HL7702的体外抑制活性;在Tris-HCl缓冲溶液中,以EB做为荧光探针,用荧光光谱法初步研究了配合物与小牛胸腺DNA的相互作用。结果表明:配合物C1、C2对5种癌细胞都有明显的抑制作用,配合物C2对HEK293、HL7702的细胞毒性远小于C1;配合物C1与小牛胸腺DNA作用是插入结合与静电结合共同作用所致,配合物C2与小牛胸腺DNA作用是插入结合作用所致。

七配位二聚体配合物{(PhCH_2)_2Sn·[2,6-(O_2C)_2C_5H_3N](CH_3OH)}_2的合成及结构

在三乙胺存在下利用三苄基氯化锡和 2 ,6 -吡啶二甲酸 ,以 1∶ 1摩尔比反应 ,合成了七配位二聚体{ ( Ph CH2 ) 2 Sn[2 ,6 -( O2 C) 2 C5H3 N]( CH3 OH) } 2 .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用 X射线单晶衍射法测定了该化合物的晶体结构 .化合物为三斜晶系 ,P1空间群 ,晶胞参数 a=0 .96 2 5 ( 6 ) nm,b=1 .0 94 7( 9) nm,c=1 .996 ( 3) nm,α=90 .0 0 ( 2 )°,β=87.6 9( 3)°,γ=90 .0 0 ( 3)°,Z=2 ,V=2 .1 0 2 ( 6 ) nm3 ,μ=1 .2 4 8mm- 1 ,F( 0 0 0 ) =1 0 0 0 ,R1 =0 .0 4 76 ,w R2 =0 .0 782 .化合物中 2个锡原子呈七配位畸变五角双锥构型 .生物活性测试结果表明 ,该化合物具有较强的体外抗肿瘤活性 .